色谱

色谱 ›› 2012, Vol. 30 ›› Issue (04): 391-394.DOI: 10.3724/SP.J.1123.2011.12060

• 特别策划 • 上一篇    下一篇

离子色谱-抑制电导检测法同时测定草甘膦母液中的含磷副产物及无机阴离子

胡忠阳*, 叶明立, 潘广文, 张婷婷, 钟乃飞   

  1. 1. 戴安中国有限公司上海实验室
    2. 戴安中国有限公司
    3. 戴安上海分析仪器有限公司
    4. 赛默飞世尔有限公司上海实验室
  • 收稿日期:2011-12-19 修回日期:2012-02-14 出版日期:2012-04-28 发布日期:2012-04-28
  • 通讯作者: 赛默飞世尔科技有限公司上海实验室, 上海 201203
  • 基金资助:

    浙江大学国家重点实验室开放基金项目(No. 2011KF07)

Simultaneous determination of phosphorous by-products and inorganic anions in glyphosate mother liquor by ion chromatography with suppressed-conductivity detection

HU Zhongyang*, YE Mingli, PAN Guangwen, ZHANG Tingting, ZHONG Naifei   

  1. Shanghai Lab., Thermo Fisher Scientific Inc., Shanghai 201203, China
  • Received:2011-12-19 Revised:2012-02-14 Online:2012-04-28 Published:2012-04-28

PDF

410

被引次数

26

摘要： 建立了一种抑制电导检测-离子色谱(IC)同时测定草甘膦生产工艺中母液里的草甘膦及其副产物、无机阴离子的方法。样品经过滤后直接进样,色谱条件: IonPac AS11-HC分离柱(250 mm×4 mm)和IonPac AG11-HC保护柱(50 mm×4 mm),在线淋洗液发生器KOH梯度淋洗,流速1.0 mL/min,采用抑制电导检测。草甘膦、甲基草甘膦、六甲基磷酰三胺(HMPA)、增甘膦、亚磷酸、磷酸、Cl~和SO2~4的线性范围分别为0.1～20 mg/L、0.1～20 mg/L、0.1～50 mg/L、0.25～50 mg/L、0.05～20 mg/L、0.2～50 mg/L、0.02～20 mg/L和0.05～50 mg/L,相关系数分别为0.9995、0.9993、0.9999、0.9998、0.9999、0.9985、0.9999和0.9980,加标回收率为93.7%～104.0%,相对标准偏差均小于2.5% (n=7),检出限(以信噪比(S/N)=3计)为0.002～0.025 mg/L。该方法用于草甘膦生产工艺中母液里草甘膦及其含磷副产物和无机阴离子的测定,结果令人满意。

关键词: 草甘膦, 含磷副产物, 离子色谱, 母液, 无机阴离子

Abstract: The by-product anion content was an important index for the evaluation of pesticide glyphosate’s productivity technology. A method was developed for the simultaneous determination of glyphosate, phosphorous by-products and other trace impurity anions in the mother liquor of glyphosate procedure by ion chromatography (IC). The sample was diluted with deionized water and filtrated by 0.22 μm nylon filter membrane, and then analyzed by IC directly without anymore pretreatment. The analytical column was Dionex IonPac AS11-HC (250 mm×4 mm) with a guard column IonPac AG11-HC (50 mm×4 mm). Gradient KOH eluent generated by an eluent generation cartridge was used at a flow rate of 1.0 mL/min. The detection was performed by a Dionex suppressed conductivity detector. The quantitative analysis of external standard calibration curves was used. The linear ranges of the method for glyphosate, methyl glyphosate, hexamethylphosphoramide (HMPA), glyphosine, phosphite, phosphate, chloride and sulfate were 0.1~20 mg/L (r=0.9995), 0.1~20 mg/L (r=0.9993), 0.1~50 mg/L (r=0.9999), 0.25~50 mg/L (r=0.9998), 0.05~20 mg/L (r=0.9999), 0.2~50 mg/L (r=0.9985), 0.02~20 mg/L (r=0.9999) and 0.05~50 mg/L (r=0.9980), respectively. The average recoveries were 93.7%~104.0% with the relative standard deviations less than 2.5% (n=7), and the detection limits (S/N=3) were 0.002~0.025 mg/L. The method has been applied to determine the contents of glyphosate, phosphorous by-products and inorganic anions in the mother liquor of glyphosate with satisfactory results.

Key words: glyphosate, inorganic anions, phosphorous by-products, ion chromatography (IC)